A kind of high-throughput preparation method of high-temperature alloy material
Technical field:
The present invention relates to high Throughput Preparation field in material genome plan, specially a kind of height of high-temperature alloy material
Flux preparation method.
Background technique:
High temperature alloy is manufacture aero-engine hot-end component critical material, and the performance of high temperature alloy plays aero-engine
To very key effect.With the raising of engine intake temperature, to high-temperature alloy material performance, more stringent requirements are proposed,
Therefore it is badly in need of the research and development higher novel high-temperature alloy material of temperature capability.In the design process of high temperature alloy composition, one important
Thinking is exactly the temperature capability for adding the refractory metal elements such as a large amount of Ta, Mo, W, Re and Ru to improve alloy.
But the raising of refractory element forms a large amount of harmful topological solid matter phases during will lead to military service
Low-alloyed high temperature creep property, seriously drops in (Topologically closedpackedphase, TCP phase).Currently, high
The design research and development of temperature alloy still rely on trial-and-error method to complete, by great wasting manpower and material resources.In recent years, China is to accelerate to close
The research and development speed of golden material realizes " double to halve " of research and development cost and period that material genome project obtains the formal vertical of country
.
Material genome project mainly include high-throughput material calculate, high-throughput material experiment and database three parts,
Polynary section is spread as the key technology in high-throughput material experiment method, has been widely used in alloying component and tissue sample
High-throughput preparation, admittedly but this method is based on consolidate/spreading phase transition process, during cannot achieve aluminium alloy/solid phase change
Prepared by ingredient and the high-throughput of tissue, using the high Throughput Preparation based on liquid/solid phase transition process, can effectively enrich high pass
Technology of preparing is measured, research and development cost and period are further decreased.
Summary of the invention:
The purpose of the present invention is to provide a kind of high-throughput preparation method of high-temperature alloy material, this method is solidifying based on alloy
Gu liquid/solid phase transformation during makes metal block or alloy block and high temperature by the control of the parameters such as directional solidification temperature and pulling rate
The generation element counterdiffusion of alloy melt is reacted, thus realize simple substance atom in the control of the diffusion length of alloy melt, thus
The control of regional area ingredient and tissue is obtained, it can be achieved that alloying component and the height for organizing the formation of with developing sample in process of setting
Flux preparation, the efficiency of high-temperature alloy material research and development can be improved using this method, reduce research and development cost and lead time.
The technical scheme is that
A kind of high-throughput preparation method of high-temperature alloy material, the specific steps are as follows:
(1) will be paraffin melting, melt paraffin injection is had in the metal die of step shape by wax injector, and keeps
It is cooled to room temperature to paraffin, forms wax-pattern;
(2) it will be sticked in having a size of the blocky adhesive plaster of 5 × 5mm~15 × 15mm and need to place the pre- of metal block or alloy block
Seated position, the position are any one face in five faces of wax-pattern top bar shape;
(3) corundum formwork is made by grout coating process in the wax-pattern combined, removes adhesive plaster after corundum formwork is made, and
The sintering of molding corundum formwork is carried out under the conditions of air atmosphere;
(4) pure metal or alloy are cut into the size being adapted with step shape using wire cutting, and removed by adhesive plaster
The metal block or alloy block preset position window formed afterwards, is placed in the corundum formwork in step (3), and using schmigel to gold
The outer surface for belonging to block or alloy block is sealed, and prevents bleed-out in experimentation;
(5) formwork with metal block or alloy block is placed in directional solidification furnace, is warming up to 1400~1600 DEG C, and will
Directional solidification is carried out after high temperature alloy melt cast to formwork.
The high-throughput preparation method of the high-temperature alloy material in step (1), paraffin is melted at 50~80 DEG C, is led to
Crossing wax injector has melt paraffin injection in the metal die of step shape, and casting pressure is 0.5~2MPa, and at room temperature
Keep 1~10min.
The high-throughput preparation method of the high-temperature alloy material, it is rigid in 850~1000 DEG C of sinter moldings in step (3)
Beautiful formwork, sintering time are 1~3 hour.
The high-throughput preparation method of the high-temperature alloy material, in step (4), using wire cutting by pure metal W, Mo,
Hf, Re or W-Al, Ni-Ti alloy are cut into the size being adapted with step shape, and the shape of metal block or alloy block is square
Or cuboid, it is mixed, is carried out using outer surface of the mixture to metal block or alloy block close with silica solution using schmigel
Envelope;In the mixture, based on mass percentage, silica solution is 5~15%, and schmigel is 85~95%.
The high-throughput preparation method of the high-temperature alloy material, in step (5), will with W, Mo, Hf, Re metal block or
The formwork of W-Al, Ni-Ti alloy block is placed in vacuum oriented consolidation furnace, is 0.01~10Pa, temperature 850~1000 in vacuum degree
DEG C sintering, to prevent metal block or alloy block from aoxidizing, heat preservation 0.5~1h, be then warming up to 1400 with 10~30 DEG C/min
~1600 DEG C, 0.5~1h is kept the temperature, and by high temperature alloy melt cast to corundum formwork, under the conditions of pulling rate is 1~9mm/min
It is oriented solidification, passes through the diffusion between casting speed control metal block or alloy block and liquid alloy.
The invention has the advantages and beneficial effects that:
1, present invention process design rationally, reserves the sky of subsequent addition metal block in traditional corundum formwork preparation process
Gap is formed using the reaction between powder in high-temperature sintering process to sky after the metal block that size is adapted is placed in gap
Gap is closed, and has the advantages that operating procedure is simple, at low cost.
2, the preparation of the liquid state diffusion idol of different-alloy is realized in the diffusion the present invention is based on element in the liquid phase.
3, operation of the present invention is simple, and rationally, strong operability can be significantly reduced and be tested in high-temperature material R&D process for design
Amount and R&D cycle and cost.
In short, the present invention, which solves multi-component diffusion section in material genome, can only realize the ingredient tissue ladder that solid/solid phase becomes
The high-throughput preparation of sample is spent, and cannot achieve the high-throughput preparation problem of liquid/solid ingredient tissue gradient sample, is advantageously implemented
China's high-temperature alloy material researches and develops the target of " double to halve " in cost and period, to accelerate the development of novel high-temperature alloy material to mention
For effective ways.
Detailed description of the invention:
Fig. 1 (a)-Fig. 1 (c) is high temperature alloy high throughput preparation structure schematic diagram;Wherein, Fig. 1 (a) is schematic three dimensional views;
Fig. 1 (b) is partial 3 d schematic diagram;Fig. 1 (c) is local X-Y scheme sectional view.
Fig. 2 (a)-(b) is the macro morphology that high temperature alloy high throughput prepares alloy.Wherein, Fig. 2 (a) Hf consecutive variations;Figure
2 (b) W consecutive variations.
Fig. 3 (a)-(e) is the micro components and microstructure evolution pattern that high temperature alloy high throughput prepares alloy.Wherein, Fig. 3
It (a) is microstructure evolution pattern;Fig. 3 (b) is Cr element;Fig. 3 (c) is Hf element;Fig. 3 (d) is W element;Fig. 3 (e) is Co element.
Specific embodiment:
As shown in Fig. 1 (a), metal block A, metal block B, metal block C, metal is respectively set in the formwork two sides of quasi- research alloy
Block D, metal block E, metal block F, side is by the arrangement of directional solidification direction metal block A, metal block B, metal block C, and the other side is by fixed
To the arrangement of solidification direction metal block D, metal block E, metal block F.
As shown in Fig. 1 (b)-Fig. 1 (c), the adhesive plaster having a size of 5 × 5~15 × 15mm is sticked in and needs to place metal block
Preset position, which can be any one face in five faces of step shape: the face A, the face B, the face C, the face D and the face E.
In the following, by embodiment, the present invention is described in more detail.
Embodiment 1
The present embodiment uses nickel base superalloy K417G alloy for research object, and the alloying component is as shown in table 1.
Main alloy element weight percent in 1 K417G alloy of table
C |
Cr |
Co |
Mo |
Al |
Ti |
V |
B |
Zr |
Ni |
0.15 |
9.0 |
10.0 |
3.0 |
5.5 |
4.5 |
0.7 |
0.015 |
0.07 |
It is remaining |
The present embodiment studies influence of the ingredient to alloy microstructure by the high-throughput preparation of high-temperature alloy material.It will
Paraffin melts at 60 DEG C, melt paraffin injected by wax injector it is pre-designed, in the metal die with step shape,
Casting pressure is 1MPa, and keeps 5min at room temperature, until paraffin solidifies completely.It will be having a size of 5 × 5mm~15 × 15mm glue
Cloth sticks in the position face A (see Fig. 1 (b)).Wax pattern combination is complete, wax-pattern will be combined by grout coating process, corundum formwork is made,
Adhesive plaster is removed after corundum formwork is made, under the conditions of formwork is placed in air atmosphere, in 900 DEG C of sinter molding corundum formworks, is burnt
Tying the time is 1.5 hours.One of pure W, Mo, Hf, Re, Nb, Cr that wire cutting is cut into etc. metal block or W-Al, Ni-Ti etc. it
One alloy block is placed in step corundum formwork, and is mixed using schmigel with silica solution, and silica solution mass ratio is in mixture
6%, schmigel mass ratio is 94%, is sealed to the outer surface of metal block or alloy block, prevents bleed-out in experimentation.It will
The formwork of preset alloy block is placed in vacuum oriented consolidation furnace, is 0.5Pa in vacuum degree, and 900 DEG C of temperature sintering keep the temperature 0.5h,
1500 DEG C then are warming up to 20 DEG C/min, keeps the temperature 0.5h, and by high temperature alloy melt cast to corundum formwork, is in pulling rate
Solidification is oriented under the conditions of 5mm/min.
Embodiment 2
The present embodiment uses nickel base superalloy K417G alloy for research object, and the alloying component is as shown in table 2.
Main alloy element weight percent in 2 K417G alloy of table
C |
Cr |
Co |
Mo |
Al |
Ti |
V |
B |
Zr |
Ni |
0.15 |
9.0 |
10.0 |
3.0 |
5.5 |
4.5 |
0.7 |
0.015 |
0.07 |
It is remaining |
The present embodiment studies influence of the ingredient to alloy microstructure by the high-throughput preparation of high-temperature alloy material.It will
Paraffin melts at 70 DEG C, melt paraffin injected by wax injector it is pre-designed, in the metal die with step shape,
Casting pressure is 1.5MPa, and keeps 6min at room temperature, until paraffin solidifies completely.It will be having a size of 5 × 5mm~15 × 15mm
Adhesive plaster sticks in the position face B (see Fig. 1 (b)).Wax pattern combination is complete, wax-pattern will be combined by grout coating process, corundum mould is made
Shell removes adhesive plaster after corundum formwork is made, under the conditions of formwork is placed in air atmosphere, in 950 DEG C of sinter molding corundum formworks,
Sintering time is 2.5 hours.One of pure W, Mo, Hf, Re, Nb, Cr that wire cutting is cut into etc. metal block or W-Al, Ni-Ti etc.
One of alloy block be placed in step corundum formwork, and mixed with silica solution using schmigel, silica solution mass ratio is in mixture
8%, schmigel mass ratio is 92%, is sealed to the outer surface of metal block or alloy block, prevents bleed-out in experimentation.It will
The formwork of preset alloy block is placed in vacuum oriented consolidation furnace, is 1.5Pa in vacuum degree, and 950 DEG C of temperature sintering keep the temperature 1h, with
1450 DEG C are warming up to 15 DEG C/min afterwards, keeps the temperature 1h, and is 3mm/ in pulling rate by high temperature alloy melt cast to corundum formwork
Solidification is oriented under the conditions of min.
Embodiment 3
The present embodiment uses nickel base superalloy K417G alloy for research object, and the alloying component is as shown in table 3.
Main alloy element weight percent in 3 K417G alloy of table
C |
Cr |
Co |
Mo |
Al |
Ti |
V |
B |
Zr |
Ni |
0.15 |
9.0 |
10.0 |
3.0 |
5.5 |
4.5 |
0.7 |
0.015 |
0.07 |
It is remaining |
The present embodiment studies influence of the ingredient to alloy microstructure by the high-throughput preparation of high-temperature alloy material.It will
Paraffin melts at 50 DEG C, melt paraffin injected by wax injector it is pre-designed, in the metal die with step shape,
Casting pressure is 0.5MPa, and keeps 3min at room temperature, until paraffin solidifies completely.It will be having a size of 5 × 5mm~15 × 15mm
Adhesive plaster sticks in the position face C (see Fig. 1 (b)).Wax pattern combination is complete, wax-pattern will be combined by grout coating process, corundum mould is made
Shell removes adhesive plaster after corundum formwork is made, under the conditions of formwork is placed in air atmosphere, in 850 DEG C of sinter molding corundum formworks,
Sintering time is 3 hours.One of pure W, Mo, Hf, Re, Nb, Cr that wire cutting is cut into etc. metal block or W-Al, Ni-Ti etc. it
One alloy block is placed in step corundum formwork, and is mixed using schmigel with silica solution, and silica solution mass ratio is in mixture
10%, schmigel mass ratio is 90%, is sealed to the outer surface of metal block or alloy block, prevents bleed-out in experimentation.
The formwork of preset alloy block is placed in vacuum oriented consolidation furnace, is 0.2Pa, 850 DEG C of temperature sintering, heat preservation in vacuum degree
0.5h is then warming up to 1550 DEG C with 25 DEG C/min, keeps the temperature 0.5h, and by high temperature alloy melt cast to corundum formwork, is drawing
Speed is oriented solidification under the conditions of being 6mm/min.
Embodiment 4
The present embodiment uses nickel base superalloy K417G alloy for research object, and the alloying component is as shown in table 4.
Main alloy element weight percent in 4 K417G alloy of table
C |
Cr |
Co |
Mo |
Al |
Ti |
V |
B |
Zr |
Ni |
0.15 |
9.0 |
10.0 |
3.0 |
5.5 |
4.5 |
0.7 |
0.015 |
0.07 |
It is remaining |
The present embodiment studies influence of the ingredient to alloy microstructure by the high-throughput preparation of high-temperature alloy material.It will
Paraffin melts at 80 DEG C, melt paraffin injected by wax injector it is pre-designed, in the metal die with step shape,
Casting pressure is 2MPa, and keeps 9min at room temperature, until paraffin solidifies completely.It will be having a size of 5 × 5mm~15 × 15mm glue
Cloth sticks in the position face D (see Fig. 1 (b)).Wax pattern combination is complete, wax-pattern will be combined by grout coating process, corundum formwork is made,
Adhesive plaster is removed after corundum formwork is made, under the conditions of formwork is placed in air atmosphere, in 1000 DEG C of sinter molding corundum formworks, is burnt
Tying the time is 1 hour.One of one of pure W, Mo, Hf, Re, Nb, Cr that wire cutting is cut into etc. metal block or W-Al, Ni-Ti etc.
Alloy block is placed in step corundum formwork, and is mixed using schmigel with silica solution, and silica solution mass ratio is 12% in mixture,
Schmigel mass ratio is 88%, is sealed to the outer surface of metal block or alloy block, prevents bleed-out in experimentation.It will be preset
The formwork of alloy block is placed in vacuum oriented consolidation furnace, is 5Pa in vacuum degree, 1000 DEG C of temperature sintering keep the temperature 1h, then with 30
DEG C/min is warming up to 1600 DEG C, 1h is kept the temperature, and be 4mm/min condition in pulling rate by high temperature alloy melt cast to corundum formwork
Under be oriented solidification.
The course of work and result of the present invention are as follows:
The present invention passes through the diffusion of atom in the liquid phase in directional solidification process under high temperature, and solving multi-component diffusion section can only
It realizes the high-throughput preparation for the ingredient tissue gradient sample that solid/solid phase becomes, and cannot achieve liquid/solid ingredient tissue gradient sample
High-throughput preparation problem is advantageously implemented the target of " double to halve " in China's high-temperature alloy material research and development cost and period, to add
The development of fast novel high-temperature alloy material provides effective ways.
As shown in Fig. 2 (a)-(b), the macro morphology for preparing alloy from high temperature alloy high throughput can be seen that no matter use
Hf ingot and W ingot, all form the tissue of consecutive variations in the alloy.
As shown in Fig. 3 (a)-(e), the micro components of alloy are prepared from high temperature alloy high throughput and microstructure evolution pattern can be with
Find out, the addition of pure metal block can change the variation of the ingredients such as Co, W, Hf and Cr in alloy, so as to cause microcosmic group of alloy
Knit the change of pattern.
Embodiment the result shows that, the present invention has preparation process simple, it is low in cost the features such as, breach the polynary section of diffusion
It can only realize that solid/solid phase gets higher flux prepared composition tissue sample.And it cannot achieve alloy graining and changed by liquid phase to solid phase
The high-throughput preparation of ingredient tissue sample in journey, especially eutectic reaction tissue, the method for the present invention can realize the group of solid-liquid phase transformation
The high-throughput preparation of tissue samples, to be conducive to high-temperature alloy material research and development.